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  3. Preparation of a new nano-sized ion template polymer for the separation and preconcentration of nickel metal ions from aqueous solutions

Preparation of a new nano-sized ion template polymer for the separation and preconcentration of nickel metal ions from aqueous solutions

Number of pages: 75 File Format: word File Code: 31860
Year: 2014 University Degree: Master's degree Category: Chemical - Petrochemical Engineering
Tags/Keywords: Ionic format - metal ions - Molecular modeling - Molecular template - nano particle - nickel - Polymer - Polymer nanoparticles - Polymerization - separation
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  • Summary of Preparation of a new nano-sized ion template polymer for the separation and preconcentration of nickel metal ions from aqueous solutions

    Master's Thesis of Analytical Chemistry

    Abstract

    In this research, the synthesis of polymer nanoparticles of ion template using sedimentation method and for the separation and preconcentration of nickel ions from aqueous samples is reported. Nickel template polymer nanoparticles by dissolving stoichiometric amount of nickel nitrate and ligand 40,20,7,5,3-pentahydroxyflavone (murine) in 23 ml of ethanol-acetonitrile (v/v 2:1) as solvent in the presence of ethylene glycol dimethacrylate as cross linker, methacrylic acid as functional monomer and azobis 2,2 Isobutyronitrile was prepared as the initiator. And then the nickel ions were washed out of the polymer using 50 ml of 6 M aqueous hydrochloric acid solution. The prepared nickel ion template polymer nanoparticles were characterized by colorimetric techniques, infrared Fourier transform and scanning electron microscope. The adsorbents obtained have a diameter between 50-70 nm and high selectivity for nickel ions in the absorption and desorption process. The nickel ions bound to the polymer were washed with 2 ml of 1.5 M hydrochloric acid solution and then their absorption was taken using a UV-Vis spectrophotometer after complexing with dimethylglyoxime (1:3). The effect of various experimental parameters on the recovery percentage of nickel ions, such as the effect of pH, absorption and washing time, initial sample volume and type, concentration and volume of detergent acid on the recovery percentage was investigated. Based on the obtained results, the highest percentage of recovery (<99%) was observed at pH=8, with an initial volume of 10 ml and absorption time of 45 minutes and desorption time of 16 minutes. In the selectivity study, it was found that the ionic template polymer shows high adsorption efficiency for nickel ions in competition with ions of the same charge and similar sizes, such as sodium (I), potassium (I), mercury (II), cobalt (II), magnesium (II, manganese (II, zinc (II), cadmium (II), copper (II), lead (II), iron (III), and chromium (III) ions). The prepared ion template polymers can be used at least 8 times was used, without a noticeable decrease in its efficiency. The polymer nanoparticles prepared in the solid phase extraction process were successfully used for the separation and preconcentration of nickel ions in water samples of Bashar Yasouj, Yasouj waterfall and drinking water of Yasouj University. 2/34 for eight measurements for a concentration of 2 mg/L of nickel.

    Key words: ion template polymer, nickel, polymerization, nanoparticles, metal ions, separation

    Chapter One

    Introduction, theory and history

    1-1- Molecular or ionic template polymers[1]

    Molecular template[2] or ionic polymers are considered important research topics of the last decade. These materials, which are also called synthetic antibodies, are made in such a way that according to the molecular characteristics of the materials, they are shaped into their mold and absorb only the desired material, and for this reason, they are also called molecular mold polymer. The exceptional properties of these materials make them suitable for use in chemical sensors, pharmaceuticals, material separation and drug measurement. These polymers are an interesting way to imitate natural molecular recognition, which is realized by preparing artificial recognition sites with high selectivity for the desired analytes. In this method, the target analyte acts as a propellant species [3] and is associated with functional monomers through covalent [4] or non-covalent bonds [5] during the process of polymer formation. The resulting fine hole polymers have recognition sites that have a high affinity for the target molecule due to the shape and arrangement of the functional groups. The selectivity and propensities obtained from the molecular modeling process are close to the selectivity and propensities of biological identification elements, such as antibodies. Molecular template technology has been introduced and developed in the past few years as a suitable alternative to various analytical methods based on natural diagnostic elements.This technique was first used as a method to create selective detection sites in synthetic polymers, and today it has found various applications. Molecular template polymers are actually a synthetic neopolymer that has a high affinity for the target molecule [1]. In fact, during the polymerization process, special networks are created to interact with the target species. In this method, first the target species forms a complex with (images are available in the main file)

    polymerizable monomers (with a carbon-carbon double bond) that have functional groups capable of interacting with the target molecule at one end, and then this complex is formed in the presence of large amounts of a cross-linking monomer[6], copolymer[7]. and therefore the shape of the complex is stabilized in the polymer. With the release of the target species from the polymer, networks will be created that are exactly complementary to the target species in terms of shape, size and orientation of the functional groups [3]. Molecule or ion recognition is a phenomenon that can be considered as a preferential binding of a molecule or ion to an acceptor with high selectivity due to close structural similarity. This concept exists precisely in molecular template polymer technology. In other words, after preparation, molecular or ionic template polymers interact only with the same primary template that is complete in every respect [4]. Artificial antibody production began. A technique invented by Dickey [8] using silica polymer to make a synthetic receptor for the colored molecules methyl orange [9] and ethyl orange [10] (Figure (1-2))[4]. Dickey found that a substance in the presence of methyl derivatives [11] is able to reabsorb that molecule 1.4 times better than the ethyl derivative [12].

    In 1952, following these results, the first chiral molding phase[13] was prepared by Corti[14] and Colombo[15].

    The first report of templated organic polymer was presented by Wolff [16] in 1972. Diglyceric acid was covalently linked to 2,32,3-vinyl benzene polymer [7] (Figure 1-3). Another major work in the field of molecular modeling was done by Mesbach [17] and his colleagues in 1984 when they introduced a new method for the formation of pre-polymerization complexes using non-covalent interactions [8]. Pattern

    The key factor in the successful synthesis of template polymers is to obtain the conditions during which the polymerization process, the target species and the monomers of the functional group have a suitable arrangement in relation to each other. Since the specific interaction of monomers and the target species are the selectivity factors of template polymers, in general there are three types of monomer interactions with the target species, these three interactions are: is a pattern Covalent bonds are chosen so that their breaking is possible after polymerization. After the dissociation stage, the functional groups interact with the templated molecule again through the formation of covalent bonds or non-covalent interactions. Some of the common covalent bonds for this purpose are carboxylic acids, braunic esters [18], ketals [19] and Schiff bases [20]. In this context, metal complexes are also involved, which can connect to the template molecules and direct them [9].

  • Contents & References of Preparation of a new nano-sized ion template polymer for the separation and preconcentration of nickel metal ions from aqueous solutions

    List:

    The first chapter. 1

    Introduction, theory and history. 1

    1-1- Molecular or ionic polymers. 1

    1-2- History. 3

    1-3- Polymer-template molecule interactions. 4

    1-3-1- covalent molding. 4

    1-3-2- non-covalent molding polymerization. 6

    1-3-3- pseudo-covalent interaction. 7

    1-4- polymer texture. 7

    1-5- ionic mold polymers. 8

    1-6- The advantages of molded polymers compared to conventional absorbents for solid phase extraction. 9

    1-7- types of molding polymer production methods. 9

    1-7-1- model molecule. 10

    1-7-2- functional monomer. 10

    1-7-3-ligand. 13

    1-7-4- starter. 13

    1-7-5-crosslinking monomer. 14

    1-8-Polymerization conditions. 14

    1-9- Polymerization methods. 15

    1-9-1- condensation polymers. 15

    1-9-2- chain polymerization reactions. 15

    1-9-2-1- bulk polymerization. 17

    1-9-2-2- solution polymerization method. 19

    1-9-2-3- Suspension polymerization 20

    1-9-2-4- Emulsion polymerization method. 20

    1-9-2-5- Sedimentation polymerization 21

    1-10- Importance and applications of molded polymers. 21

    1-10-1- Separation. 22

    1-10-2- Membrane construction. 23

    1-10-3- Making sensor or electrode. 24

    1-10-4- synthetic receptors. 25

    1-10-5- Catalysts 25

    1-11- Nickel element. 26

    1-12- Review of past works. 27

    The second chapter. 30

    Experimental part. 30

    2-1- Required devices and equipment. 30

    2-2- Necessary chemicals. 30

    2-3- Synthesis of ion template polymer nanoparticles for nickel ion measurement. 32

    2-4- Synthesis of unmolded polymer. 33

    2-5-Solution. 33

    2-5-1- Preparation of necessary solutions to check the formation and determine the ratio of metal to ligand complex. 33

    2-5-2- Preparation of mother nickel solution. 33

    2-5-3- preparation of dimethylglyoxime mother solution for spectrophotometric measurement. 34

    2-5-4- Preparation of solutions of different cations to investigate the effects of disturbance. 34

    2-6- Preparation of water samples for nickel measurement. 34

    2-7- Preconcentration of nickel ion using prepared ion template polymers. 34

    The third chapter. 36

    Checking the results and conclusions. 36

    3-1- Investigating the formation and determining the ratio of metal to ligand complex between nickel ion and murine. 36

    3-2- Properties of nickel ion mold polymer. 39

    3-2-1- Colorimetry. 39

    3-2-2- FT-IR spectrum of nickel ion mold polymer. 39

    3-2-3- electron microscope image. 40

    3-3- Preconcentration and separation of nickel ions using synthesized ion template polymers. 42

    3-3-1- Examining the effect of pH on extraction. 42

    3-3-2- Checking the amount of absorbent. 44

    3-3-3- Examining the effect of the type of detergent acid. 44

    3-3-4- Examining the effect of detergent acid concentration. 45

    3-3-5- Investigating the effect of detergent acid volume. 45

    3-3-6- Examining the effect of time on the absorption and desorption process of nickel ions. 48

    3-3-7- The initial volume of the sample and calculation of the final limit of dilution. 49

    3-3-8- Studying the frequency of use of polymer nano particles of ion mold. 50

    3-3-8- absorption capacity. 51

    3-3-9- Figures of merit of the method. 52

    3-3-10- Linear range. 52

    . 3-3-11- detection limit of the method. 53

    3-3-12- selectivity of the method. 54

    3-3-13- Reproducibility of the method. 55

    3-3-14- Application of the present method for preconcentration and measurement of nickel ion in water samples. 55

    3-4- Conclusion and future perspective. 58

    Resources: 60

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